CN110735120A - NbN/MoSN/MoS2Hard self-lubricating nano-structure composite film and preparation method thereof - Google Patents

NbN/MoSN/MoS2Hard self-lubricating nano-structure composite film and preparation method thereof Download PDF

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CN110735120A
CN110735120A CN201911051514.9A CN201911051514A CN110735120A CN 110735120 A CN110735120 A CN 110735120A CN 201911051514 A CN201911051514 A CN 201911051514A CN 110735120 A CN110735120 A CN 110735120A
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鞠洪博
喻利花
许俊华
汪然
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Jiangsu University of Science and Technology
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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Abstract

The invention discloses NbN/MoSN/MoS2The hard self-lubricating nano-structure composite film is prepared by using Nb as a transition layer, adopting a radio frequency magnetron sputtering technology, and using a high-purity Nb target and high-purity MoS2The film is prepared by target confocal sputtering, has the thickness of 1.5-2 mu m and consists of face-centered cubic NbN, close-packed hexagonal NbN, amorphous MoSN and MoS2In which the crystalline NbN is replaced by amorphous MoSN and MoS2And (4) wrapping to show the microstructure characteristic of amorphous wrapped nanocrystalline. The NbN/MoSN/MoS2The nano-structure composite film has high hardness and excellent room-temperature friction and wear performance; the preparation method of the composite membrane has the advantages of simple process flow and high production efficiency; the composite film can be used for high-performance dry cutting tool film materials and working diesA film material having improved surface properties.

Description

NbN/MoSN/MoS2Hard self-lubricating nano-structure composite film and preparation method thereof
Technical Field
The invention relates to an inorganic nitride-based ceramic film and preparation thereof, in particular to NbN/MoSN/MoS2A hard self-lubricating nano-structure composite film and a preparation method thereof.
Background
However, with the rapid development of modern processing technology, more severe requirements are provided for the service performance of high-end cutting tools and dies, and the requirements comprise higher hardness, stronger friction reduction and wear resistance, and the like, the traditional binary niobium nitride film material is difficult to completely meet the performance requirements.
Disclosure of Invention
The invention aims to provide NbN/MoSN/MoS2The hard self-lubricating nano-structure composite film and the preparation method solve the problem that the prior binary niobium nitride film material can not meet the service performance requirement of high-end cutting tools.
The technical scheme is as follows: the NbN/MoSN/MoS2The hard self-lubricating nano-structure composite film comprises an Nb transition layer, wherein the Nb transition layer is provided with NbN/MoSN/MoS2A composite film layer of said NbN/MoSN/MoS2The composite film layer comprises face-centered cubic NbN, close-packed hexagonal NbN, amorphous MoSN and MoS2In which the crystalline NbN is substituted by the amorphous phases MoSN and MoS2And (6) packaging.
Wherein the thickness of the Nb transition layer is 50-400 nm.
The NbN/MoSN/MoS2The atomic percentage content ranges of Nb, Mo, S and N in the composite film layer are 12.7-60.4, 3.7-23.4, 4.5-27.8 and 31.4-36.1 at.% in sequence.
The NbN/MoSN/MoS2The nano-structure composite film has the hardness of 18-25GPa, the average friction coefficient at room temperature of 0.61-0.32 and the wear rate at room temperature of 1.7 multiplied by 10-8-3.2×10-7mm3·N-1mm-1。
The NbN/MoSN/MoS2The thickness of the nanostructure composite film is 1.5-2 μm.
The NbN/MoSN/MoS2The preparation method of the hard self-lubricating nano-structure composite membrane comprises the following steps:
(1) the substrate material is sequentially ultrasonically cleaned in acetone and alcohol for 10-15 minutes, and then dried by hot air and placed on a clamp of a magnetron sputtering chamber. Placing high-purity Nb target and MoS on a radio frequency sputtering gun in a sputtering chamber2A target;
(2) the background vacuum degree of the chamber to be sputtered is lower than 6.0 multiplied by 10-4When Pa is needed, high-purity Ar gas is introduced, and the high-purity Nb target and the MoS are ignited2After the target, the air pressure is adjusted to 0.3Pa, and the high-purity Nb target and MoS are adjusted2The power of a target radio frequency power supply is 30W, and pre-sputtering is carried out for 15 minutes to remove pollutants on the surface of the target;
(3) shutdown MoS2The target baffle plate is used for opening the substrate baffle plate after the power of the Nb target is adjusted to 150W, and sputtering an Nb transition layer on the substrate;
(4) introducing high-purity nitrogen, fixing the Nb target power at 150W and the flow ratio of the argon to the nitrogen at 10:5, and adjusting MoS2The target power is 30-130W, and NbN/MoSN/MoS is prepared2A composite membrane.
Has the advantages that: the invention has good mechanical and tribological properties; the preparation method has the advantages of simple process flow and high production efficiency; the invention can be used for high-performance dry cutting tool film materials and film materials with improved tool and die surface properties.
Drawings
FIG. 1 is a binary NbN thin film XRD pattern;
FIG. 2 is a high resolution TEM image of the composite film of example 5;
FIG. 3 is a graph showing the average coefficient of friction at room temperature of the films in the examples;
FIG. 4 is a graph showing the film wear rate at room temperature for each example.
Detailed Description
The invention is further illustrated in the following description with reference to the figures and examples.
Firstly, preparing a binary NbN film as a comparative example, wherein the thickness of the binary NbN film is between 1.5 and 2 mu m, and niobium with the thickness of 400nm is selected as a transition layer. NbN as shown in FIG. 1The XRD pattern of the film shows that the film consists of face-centered cubic NbN and close-packed hexagonal NbN, and the chemical formula of the film can be expressed as NbNx. The relative atomic percent of Nb and N in the film was 67.3, 32.7 at.%, respectively. The film hardness is about 28GPa, and the average friction coefficient and the wear rate at room temperature are respectively 0.68 and 6.7 multiplied by 10-7mm3·N-1mm-1。
The preparation method of the binary NbN film comprises the following steps:
(1) sequentially ultrasonically cleaning substrate materials such as stainless steel, ceramics and high-speed steel in acetone and alcohol for 15 minutes, blow-drying the substrate materials by hot air, placing the substrate materials on a fixture of a magnetron sputtering chamber, and placing a high-purity Nb target and MoS on a radio-frequency sputtering gun in the sputtering chamber2The diameter of the target and the diameter of the target are both 75mm, and the thickness of the target is 20 mm.
(2) The background vacuum degree of the chamber to be sputtered is better than 6.0 multiplied by 10-4When Pa is needed, high-purity Ar gas is introduced, after the high-purity molybdenum target and the molybdenum sulfide target are ignited, the gas pressure is adjusted to 0.3Pa, and the high-purity Nb target and the MoS are adjusted2The power of the target radio frequency power supply is 30W, and pre-sputtering is carried out for 15 minutes to remove the pollutants on the surface of the target.
(3) And closing the molybdenum sulfide target baffle, adjusting the power of the Nb target to 150W, opening the substrate baffle, and sputtering an Nb transition layer of 50-400nm on the substrate to improve the film-substrate bonding force.
(4) Introducing high-purity nitrogen, and fixing the Nb target and the MoS2The power is 150W and 0W respectively, the flow ratio of argon to nitrogen is 10:5, and the NbN composite film is prepared.
The following preparation of NbN/MoSN/MoS with different proportions2The film material comprises the following specific components:
example 1
The basic procedure was the same as for the preparation of binary NbN films, except that after the Nb transition layer was deposited, the MoS was adjusted2The target power was 30W. The composite membrane in this example has a thickness of about 1.5-2 μm. The atomic percentage of Nb, Mo, S and N in the composite film is 60.4, 3.7, 4.5 and 31.4 at.% in sequence. The composite film is composed of face-centered cubic NbN, close-packed hexagonal NbN, amorphous MoSN and MoS2In which the crystalline NbN is replaced by amorphous MoSN and MoS2Wrap up to present an "amorphous wrap upNanocrystalline "microstructure characteristics. The composite film has a hardness of about 25GPa, and average friction coefficient and wear rate of 0.61 and 3.2 × 10 at room temperature-7mm3·N-1mm-1。
Example 2
The basic procedure was the same as for the preparation of binary NbN films, except that after the Nb transition layer was deposited, the MoS was adjusted2The target power is 60W. The composite membrane in this example has a thickness of about 1.5-2 μm. The atomic percentage of Nb, Mo, S and N in the composite film is 51.4, 6.7, 9.4 and 32.5 at.% in sequence. The composite film is composed of face-centered cubic NbN, close-packed hexagonal NbN, amorphous MoSN and MoS2In which the crystalline NbN is replaced by amorphous MoSN and MoS2And (4) wrapping to show the microstructure characteristic of amorphous wrapped nanocrystalline. The composite film has a hardness of about 21GPa, and average friction coefficient and wear rate of 0.53 and 8.5 × 10 at room temperature-8mm3·N-1mm-1。
Example 3
The basic procedure was the same as for the preparation of binary NbN films, except that after the Nb transition layer was deposited, the MoS was adjusted2The target power is 90W. The composite membrane in this example has a thickness of about 1.5-2 μm. The atomic percentage contents of Nb, Mo, S and N in the composite film are 42.1, 10.4, 13.8 and 33.7 at.% in sequence. The composite film is composed of face-centered cubic NbN, close-packed hexagonal NbN, amorphous MoSN and MoS2In which the crystalline NbN is replaced by amorphous MoSN and MoS2And (4) wrapping to show the microstructure characteristic of amorphous wrapped nanocrystalline. The composite film has a hardness of about 19GPa, and average friction coefficient and wear rate of 0.43 and 5.9 × 10 at room temperature-8mm3·N-1mm-1。
Example 4
The basic procedure was the same as for the preparation of binary NbN films, except that after the Nb transition layer was deposited, the MoS was adjusted2The target power is 110W. The composite membrane in this example has a thickness of about 1.5-2 μm. The atomic percentage of Nb, Mo, S and N in the composite film is 29.3, 17.2, 19.3 and 34.2 at.% in sequence. The composite film is composed of face-centered cubic NbN, close-packed hexagonal NbN, amorphous MoSN and MoS2In which the crystalline NbN is amorphousMoSN and MoS2And (4) wrapping to show the microstructure characteristic of amorphous wrapped nanocrystalline. The composite film has a hardness of about 18GPa, and average friction coefficient and wear rate of 0.33 and 1.9X 10 at room temperature-8mm3·N-1mm-1。
Example 5
The basic procedure was the same as for the preparation of binary NbN films, except that after the Nb transition layer was deposited, the MoS was adjusted2Target power 130W. The composite membrane in this example has a thickness of about 1.5-2 μm. The atomic percentage contents of Nb, Mo, S and N in the composite film are 12.7, 23.4, 27.8 and 36.1 at.% in sequence. The composite film is composed of face-centered cubic NbN, close-packed hexagonal NbN, amorphous MoSN and MoS2In which the crystalline NbN is replaced by amorphous MoSN and MoS2And (4) wrapping to show the microstructure characteristic of amorphous wrapped nanocrystalline. The composite film has a hardness of about 18GPa, and average friction coefficient and wear rate of 0.32 and 1.7 × 10 at room temperature-8mm3·N-1mm-1。
The composite film obtained in example 5 was subjected to transmission electron microscopy and the results are shown in FIG. 2, from which it can be seen that the composite film consisted of crystalline NbN and amorphous MoSN and MoS2In which the crystalline NbN is replaced by amorphous MoSN and MoS2And (4) wrapping to show the microstructure characteristic of amorphous wrapped nanocrystalline.
The friction coefficient test and the wear rate test were performed on the composite films of examples 1 to 5, and the results are shown in fig. 3 and 4, from which it can be seen that: average coefficient of friction of composite films with MoS2The increase of the atom percentage content is gradually reduced; wear rate of composite membranes with MoS2The increase in atomic percentage gradually decreased, indicating MoS2Has good antifriction effect on the composite film.

Claims (6)

1, NbN/MoSN/MoS2The hard self-lubricating nano-structure composite film is characterized by comprising an Nb transition layer, wherein the Nb transition layer is provided with NbN/MoSN/MoS2A composite film layer of said NbN/MoSN/MoS2The composite film layer comprises face-centered cubic NbN, close-packed hexagonal NbN, amorphous MoSN and MoS2In which the crystalline NbN is substituted by the amorphous phases MoSN and MoS2And (6) packaging.
2. NbN/MoSN/MoS according to claim 12The hard self-lubricating nano-structure composite film is characterized in that the thickness of the Nb transition layer is 50-400 nm.
3. NbN/MoSN/MoS according to claim 12The hard self-lubricating nano-structure composite film is characterized in that the NbN/MoSN/MoS2The atomic percentage content ranges of Nb, Mo, S and N in the composite film layer are 12.7-60.4, 3.7-23.4, 4.5-27.8 and 31.4-36.1 at.% in sequence.
4. NbN/MoSN/MoS according to claim 12The hard self-lubricating nano-structure composite film is characterized in that the NbN/MoSN/MoS2The nano-structure composite film has the hardness of 18-25GPa, the average friction coefficient at room temperature of 0.61-0.32 and the wear rate at room temperature of 1.7 multiplied by 10-8-3.2×10-7mm3·N-1mm-1。
5. NbN/MoSN/MoS according to claim 12The hard self-lubricating nano-structure composite film is characterized in that the NbN/MoSN/MoS2The thickness of the nanostructure composite film is 1.5-2 μm.
6. The NbN/MoSN/MoS of any of claims 1-5 to 2The preparation method of the hard self-lubricating nano-structure composite film is characterized by comprising the following steps of:
(1) the substrate material is sequentially ultrasonically cleaned in acetone and alcohol for 10-15 minutes, and then dried by hot air and placed on a clamp of a magnetron sputtering chamber. Placing high-purity Nb target and MoS on a radio frequency sputtering gun in a sputtering chamber2A target;
(2) the background vacuum degree of the chamber to be sputtered is lower than 6.0 multiplied by 10-4When Pa is needed, high-purity Ar gas is introduced, and the high-purity Nb target and the MoS are ignited2After the target, the air pressure is adjusted to 0.3Pa, and the high-purity Nb target and MoS are adjusted2Target shootingThe power of a frequency power supply is 30W, and pre-sputtering is carried out for 15 minutes to remove pollutants on the surface of the target material;
(3) shutdown MoS2The target baffle plate is used for opening the substrate baffle plate after the power of the Nb target is adjusted to 150W, and sputtering an Nb transition layer on the substrate;
(4) introducing high-purity nitrogen, fixing the Nb target power at 150W and the flow ratio of the argon to the nitrogen at 10:5, and adjusting MoS2The target power is 30-130W, and NbN/MoSN/MoS is prepared2A composite membrane.
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CN111876732A (en) * 2020-06-17 2020-11-03 西安交通大学 Molybdenum boron nitride/molybdenum sulfide nano composite coating and preparation method thereof

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CN109778130A (en) * 2019-01-21 2019-05-21 天津职业技术师范大学(中国职业培训指导教师进修中心) AlCrN/MoS with self-lubricating and wear-resisting property2Nano compound film and preparation method thereof

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CN1846990A (en) * 2005-04-13 2006-10-18 日立金属株式会社 Multi-layer coating having excellent adhesion and sliding properties and production method thereof
CN101787518A (en) * 2010-03-24 2010-07-28 中国地质大学（北京） Multi-ion-beam sputter-deposition technology for doping with diamond-like carbon (DLC) coating
CN104002516A (en) * 2014-06-10 2014-08-27 上海理工大学 CrAlN/MoS2 multi-layered coating layer with high rigidity and low friction coefficient and preparation method thereof
CN104029435A (en) * 2014-06-10 2014-09-10 上海理工大学 NbN/WS2 multilayer coating with high hardness and low friction coefficient and preparation method thereof
CN105779951A (en) * 2014-12-25 2016-07-20 中国科学院兰州化学物理研究所 Preparation method of MoS2/NbC/DLC multi-element nanocomposite super-lubricating thin film
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CN108754416A (en) * 2018-05-28 2018-11-06 苏州市启献智能科技有限公司 A kind of the low abrasion guide rod and its surface treatment of pneumatic actuator application
CN109778130A (en) * 2019-01-21 2019-05-21 天津职业技术师范大学(中国职业培训指导教师进修中心) AlCrN/MoS with self-lubricating and wear-resisting property2Nano compound film and preparation method thereof

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CN111876732A (en) * 2020-06-17 2020-11-03 西安交通大学 Molybdenum boron nitride/molybdenum sulfide nano composite coating and preparation method thereof
CN111876732B (en) * 2020-06-17 2023-06-06 西安交通大学 Molybdenum boride/molybdenum sulfide nano composite coating and preparation method thereof

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